CN113149613A - ITWO target material and preparation method thereof - Google Patents
ITWO target material and preparation method thereof Download PDFInfo
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- CN113149613A CN113149613A CN202110568300.XA CN202110568300A CN113149613A CN 113149613 A CN113149613 A CN 113149613A CN 202110568300 A CN202110568300 A CN 202110568300A CN 113149613 A CN113149613 A CN 113149613A
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Abstract
The invention discloses an ITWO target material, and relates to the field of target material preparation. The ITWO target material comprises a metal oxide composition, wherein the metal oxide composition comprises the following components: indium oxide, tin oxide, and tungsten oxide; tungsten oxide accounts for 1-5% of the total mass of the indium oxide and the tin oxide; the preparation process of the ITWO target material comprises the following steps: and (3) forming the oxidized metal composition compact and sintering. According to the invention, tungsten oxide is doped into the ITO slurry, so that the performance of the film is better, and the target material density is improved through stage sintering.
Description
Technical Field
The invention relates to the field of target preparation, in particular to an ITWO target and a preparation method thereof.
Background
The high-performance thin film material is applied to various high-end electronic industries. Amorphous Oxide Semiconductors (AOS) are widely considered as an active layer material of Thin Film Transistors (TFTS) that can replace conventional Amorphous silicon as a next generation display technology. The oxide Thin Film Transistor (TFT) active layer prepared by magnetron sputtering has good stability, can meet the requirements of high-resolution LCD, AMOLED, electronic paper and other high-end display, and has the advantages of simple process, low cost, good uniformity and the like compared with the LTPS active layer.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide the ITWO target material with the relative density of more than 95%, the target material purity of 99.99%, the average grain size of 10-15 um and the bending strength of more than or equal to 80MPa and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: an ITWO target comprising an oxidized metal composition comprising the following components: indium oxide, tin oxide, and tungsten oxide; tungsten oxide accounts for 1-5% of the total mass of the indium oxide and the tin oxide; the preparation process of the ITWO target material comprises the following steps: and (3) forming the oxidized metal composition compact and sintering.
The ITWO target material is obtained by matching indium oxide, tin oxide and tungsten oxide and performing molding sintering. The ITWO target material prepared by the invention has the relative density of more than 95%, the target material purity of 99.99%, the average grain size of 10-15 um and the bending strength of more than or equal to 80 MPa. According to the invention, tungsten oxide is doped into the ITO slurry, so that the performance of the film is better, and the target material density is improved through stage sintering.
Preferably, the mass ratio of the indium oxide to the tin oxide is: indium oxide: tin oxide is 9: 1.
Further, the application provides a preparation method of the ITWO target material, which comprises the following steps:
(1) mixing indium oxide and tin oxide according to a mass ratio, adding deionized water, and performing ball milling to obtain ITO slurry; adding tungsten oxide with corresponding mass into deionized water, and performing ball milling to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder and a pH regulator, uniformly stirring to obtain mixed slurry, and drying to obtain ITWO powder;
(3) and forming an ITWO powder compact to obtain a biscuit, and sequentially carrying out degreasing sintering, aerobic sintering and anaerobic sintering on the biscuit to obtain the ITWO target material.
Preferably, in the step (1), the ITO paste has D50<0.5 μm and a half-peak width < 0.5.
Preferably, in the step (2), the mass of the binder is 2-5% of the total mass of the tungsten oxide and ITO mixed slurry, and the binder is a polyvinyl alcohol binder; the pH regulator is ammonia water, and the pH value of the mixed slurry after regulation is 9-10.
Preferably, in the step (2), the drying mode is spray drying; the drying temperature of spray drying is 240-260 ℃, and the feeding speed is 600-1000 mL/min; the particle size of the obtained ITWO powder is less than 200 microns, and the moisture content of the ITWO powder is 0.2-0.3%.
Preferably, in the step (3), the process of forming the compact is as follows: putting ITWO powder into a die, pressing at 50MPa, and cold isostatic pressing at 300-400MPa to obtain the product with density of 4.2-4.5g/cm3The biscuit of (1).
Preferably, in the step (3), the degreasing and sintering process is as follows: placing the biscuit in a sintering furnace, heating to 150-400 ℃ at the heating rate of 0.1-0.5 ℃/min, and carrying out degreasing sintering at the oxygen flow of 50-100L/min;
the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 500-1300 ℃ at the heating rate of 0.1-0.5 ℃/min to carry out multi-stage heat preservation and sintering, and preserving heat for 1-4h at each temperature stage; heating to 1580 ℃ of 1300 ℃ at the heating rate of 0.3-0.5 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat preservation time of each temperature stage is 2-8 h; introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 50-100L/min;
the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.2-0.5 ℃/min, and preserving heat for 2-3 hours; heating to the highest target temperature at a heating rate of 0.1-0.3 ℃/min, preserving heat for 3-5 hours, then cooling to 25 ℃ at a cooling rate of 1-3 ℃/min, and introducing no gas in the process;
the multi-stage heat preservation sintering comprises a plurality of temperature rising stages and heat preservation stages, the temperature rises sequentially, and the temperature difference between any two heat preservation stages is 50-400 ℃.
After a large amount of experimental researches, the inventor of the application finds that degreasing sintering is to sinter and volatilize various lipid additives in the target material, the oxygen sintering changes the results of three oxide crystals, and tungsten atoms and tin atoms are doped into the results of the indium oxide crystals to form the ITWO target material. The target material is subjected to anaerobic sintering again after being cooled to 1400 ℃, so that the density of the target material is more compact, and compared with secondary sintering, the process has the advantages of saving time and cost from room temperature to 1400 ℃, and improving the production efficiency.
Preferably, the maximum target temperature during the oxygen-free sintering is 1500-.
Compared with the prior art, the invention has the beneficial effects that: (1) the ITWO target material is obtained by matching indium oxide, tin oxide and tungsten oxide and performing molding sintering. (2) The ITWO target material prepared by the invention has the relative density of more than 95%, the target material purity of 99.99%, the average grain size of 10-15 um and the bending strength of more than or equal to 80 MPa. (3) According to the invention, tungsten oxide is doped into the ITO slurry, so that the performance of the film is better, and the target material density is improved through stage sintering.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
In an embodiment of the present invention, the method for preparing an ITWO target according to the embodiment includes the following steps:
(1) mixing indium oxide and tin oxide according to a mass ratio (indium oxide: tin oxide is 9:1), adding deionized water, and performing ball milling for 4 hours to obtain ITO slurry, wherein the solid content (mass) of the ITO slurry is 60%; adding tungsten oxide (tungsten oxide accounts for 3% of the total mass of indium oxide and tin oxide) with corresponding mass into deionized water, and performing ball milling for 1h to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder (polyvinyl alcohol, the mass of the polyvinyl alcohol is 3% of the total mass of the tungsten oxide and ITO mixed slurry) and a pH regulator, uniformly stirring to obtain mixed slurry, stirring for 3 hours, and performing spray drying at the spray drying temperature of 250 ℃ at the feeding speed of 600mL/min, wherein the pH value of the mixed slurry is 9-10; the obtained ITWO powder has the particle size of less than 200 microns, and the water content of the ITWO powder is 0.2-0.3%;
(3) forming an ITWO powder pressed compact to obtain a biscuit, wherein the pressed compact forming process comprises the following steps: putting ITWO powder into a die, pressing at 50MPa, cold isostatic pressing at 300MPa to obtain a density of 4.2-4.5g/cm3The biscuit of (1); the biscuit is subjected to degreasing sintering, aerobic sintering and anaerobic sintering in sequence, and the degreasing sintering process comprises the following steps: placing the biscuit in a sintering furnace, heating to 150 and 400 ℃ at the heating rate of 0.3 ℃/min, and carrying out degreasing sintering;
the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 800 ℃, 1100 ℃ and 1250 ℃ at the heating rate of 0.25 ℃/min, and carrying out multi-stage heat preservation and sintering, wherein the heat preservation time of each temperature stage is 2 hours; heating to 1300 ℃ and 1400 ℃ at the heating rate of 0.3 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat preservation time of each temperature stage is 2 hours; heating to 1580 ℃ at the heating rate of 0.3 ℃/min, and preserving heat for 8 hours; introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 50-100L/min;
the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.3 ℃/min, and preserving heat for 2 hours; heating to 1550 deg.C at a rate of 0.1 deg.C/min, maintaining for 5 hr, cooling to 1000 deg.C at a rate of 1 deg.C/min, and cooling to 25 deg.C at a rate of 3 deg.C/min, wherein no gas is introduced during the process; and finally obtaining the ITWO target material.
Example 2
In an embodiment of the present invention, the method for preparing an ITWO target according to the embodiment includes the following steps:
(1) mixing indium oxide and tin oxide according to a mass ratio (indium oxide: tin oxide is 9:1), adding deionized water, and performing ball milling for 4 hours to obtain ITO slurry, wherein the solid content (mass) of the ITO slurry is 60%; adding tungsten oxide (tungsten oxide accounts for 5% of the total mass of indium oxide and tin oxide) with corresponding mass into deionized water, and performing ball milling for 1h to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder (polyvinyl alcohol, the mass of the polyvinyl alcohol is 5% of the total mass of the tungsten oxide and ITO mixed slurry) and a pH regulator, uniformly stirring to obtain mixed slurry, stirring for 5 hours, and performing spray drying, wherein the drying temperature of the spray drying is 250 ℃, and the feeding speed is 700mL/min, wherein the pH value of the mixed slurry is 9-10; the obtained ITWO powder has the particle size of less than 200 microns, and the water content of the ITWO powder is 0.2-0.3%;
(3) forming an ITWO powder pressed compact to obtain a biscuit, wherein the pressed compact forming process comprises the following steps: putting ITWO powder into a die, pressing at 50MPa, and cold isostatic pressing at 350MPa to obtain a density of 4.2-4.5g/cm3The biscuit of (1); the biscuit is subjected to degreasing sintering, aerobic sintering and anaerobic sintering in sequence, and the degreasing sintering process comprises the following steps: placing the biscuit in a sintering furnace, heating to 150 and 400 ℃ at the heating rate of 0.3 ℃/min, and carrying out degreasing sintering; the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 1000 ℃, 1100 ℃ and 1200 ℃ at the heating rate of 0.3 ℃/min, and carrying out multi-stage heat preservation and sintering, wherein the heat preservation time is 3 hours in each temperature stage; heating to 1300 ℃, 1350 ℃, 1400 ℃ and 1450 ℃ at the heating rate of 0.25 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat is preserved for 3h in each temperature stage; finally, heating to 1580 ℃, and sintering for 8 hours under heat preservation; introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 50L/min; the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.2 ℃/min, and preserving heat for 3 hours; heating to 1580 ℃ at the heating rate of 0.15 ℃/min, preserving heat for 5 hours, then cooling to 800 ℃ at the cooling rate of 1 ℃/min, and then cooling to 25 ℃ at the cooling rate of 3 ℃/min, wherein no gas is introduced in the process; and finally obtaining the ITWO target material.
Example 3
In an embodiment of the present invention, the method for preparing an ITWO target according to the embodiment includes the following steps:
(1) mixing indium oxide and tin oxide according to a mass ratio (indium oxide: tin oxide is 9:1), adding deionized water, and performing ball milling for 3 hours to obtain ITO slurry, wherein the solid content (mass) of the ITO slurry is 60%; adding tungsten oxide (tungsten oxide accounts for 2% of the total mass of indium oxide and tin oxide) with corresponding mass into deionized water, and performing ball milling for 1h to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder (polyvinyl alcohol, the mass of the polyvinyl alcohol is 4% of the total mass of the tungsten oxide and ITO mixed slurry) and a pH regulator, uniformly stirring to obtain mixed slurry, stirring for 5 hours, and performing spray drying, wherein the drying temperature of the spray drying is 250 ℃, and the feeding speed is 700mL/min, wherein the pH value of the mixed slurry is 9-10; the obtained ITWO powder has the particle size of less than 200 microns, and the water content of the ITWO powder is 0.2-0.3%;
(3) forming an ITWO powder pressed compact to obtain a biscuit, wherein the pressed compact forming process comprises the following steps: putting ITWO powder into a die, pressing at 50MPa, cold isostatic pressing at 380MPa to obtain the product with density of 4.2-4.5g/cm3The biscuit of (1); the biscuit is subjected to degreasing sintering, aerobic sintering and anaerobic sintering in sequence, and the degreasing sintering process comprises the following steps: placing the biscuit in a sintering furnace, heating to 150 and 400 ℃ at the heating rate of 0.4 ℃/min, and carrying out degreasing sintering; the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 1000 ℃, 1100 ℃ and 1200 ℃ at the heating rate of 0.3 ℃/min, and carrying out multi-stage heat preservation and sintering, wherein the heat preservation time is 3 hours in each temperature stage; heating to 1300 ℃, 1350 ℃, 1400 ℃ and 1450 ℃ at the heating rate of 0.25 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat is preserved for 3h in each temperature stage; finally heating to 1580 ℃, and sintering for 8 hours under heat preservation;
introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 50L/min; the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.3 ℃/min, and preserving heat for 3 hours; heating to 1560 ℃ at the heating rate of 0.2 ℃/min, preserving heat for 4 hours, then cooling to 1200 ℃ at the cooling rate of 1 ℃/min, and then cooling to 25 ℃ at the cooling rate of 3 ℃/min, wherein no gas is introduced in the process; and finally obtaining the ITWO target material.
Example 4
In an embodiment of the present invention, the method for preparing an ITWO target according to the embodiment includes the following steps:
(1) mixing indium oxide and tin oxide according to a mass ratio (indium oxide: tin oxide is 9:1), adding deionized water, and performing ball milling for 4 hours to obtain ITO slurry, wherein the solid content (mass) of the ITO slurry is 60%; adding tungsten oxide (tungsten oxide accounts for 1% of the total mass of indium oxide and tin oxide) with corresponding mass into deionized water, and performing ball milling for 1h to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder (polyvinyl alcohol, the mass of the polyvinyl alcohol is 5% of the total mass of the tungsten oxide and ITO mixed slurry) and a pH regulator, uniformly stirring to obtain mixed slurry, stirring for 5 hours, and performing spray drying, wherein the drying temperature of the spray drying is 250 ℃, and the feeding speed is 700mL/min, wherein the pH value of the mixed slurry is 9-10; the obtained ITWO powder has the particle size of less than 200 microns, and the water content of the ITWO powder is 0.2-0.3%;
(3) forming an ITWO powder pressed compact to obtain a biscuit, wherein the pressed compact forming process comprises the following steps: putting ITWO powder into a die, pressing at 50MPa, and cold isostatic pressing at 400MPa to obtain a density of 4.2-4.5g/cm3The biscuit of (1); the biscuit is subjected to degreasing sintering, aerobic sintering and anaerobic sintering in sequence, and the degreasing sintering process comprises the following steps: placing the biscuit in a sintering furnace, heating to 150 and 400 ℃ at the heating rate of 0.2 ℃/min, and carrying out degreasing sintering; the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 1000 ℃, 1100 ℃ and 1200 ℃ at the heating rate of 0.3 ℃/min, and carrying out multi-stage heat preservation and sintering, wherein the heat preservation time is 3 hours in each temperature stage; heating to 1300 ℃, 1350 ℃, 1450 ℃ and 1500 ℃ at the heating rate of 0.25 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat preservation time of each temperature stage is 4 h; finally heating to 1580 ℃, preserving heat and sintering for 8 hours,
introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 100L/min; the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.5 ℃/min, and preserving heat for 2 hours; heating to 1580 ℃ at the heating rate of 0.3 ℃/min, preserving heat for 5 hours, then cooling to 1000 ℃ at the cooling rate of 2 ℃/min, and then cooling to 25 ℃ at the cooling rate of 3 ℃/min, wherein no gas is introduced in the process; and finally obtaining the ITWO target material.
Comparative examples 1-3 are provided herein, and specific comparative examples 1-3 are provided as follows:
comparative example 1 compared with example 1, the mass ratio of indium oxide and tin oxide in only step (1) was different, and the mass ratio of indium oxide and tin oxide was: indium oxide: tin oxide 97:3, the rest of the preparation method is completely the same as that of example 1;
comparative example 2 compared with example 1, the mass ratio of indium oxide and tin oxide in step (1) alone was different, and the mass ratio of indium oxide and tin oxide was: indium oxide: tin oxide 95:5, the rest of the preparation method is completely the same as that of the example 1;
comparative example 3 compared with example 1, only sintering manner in step (3) is different, and the rest of preparation method is completely the same as example 1; sequentially carrying out degreasing sintering and aerobic sintering on the biscuit without carrying out anaerobic sintering to obtain the ITWO target material;
wherein, the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 800 ℃, 1100 ℃ and 1250 ℃ at the heating rate of 0.25 ℃/min, and carrying out multi-stage heat preservation and sintering, wherein the heat preservation time of each temperature stage is 2 hours; heating to 1300 ℃ and 1400 ℃ at the heating rate of 0.3 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat preservation time of each temperature stage is 2 hours; heating to 1580 ℃ at the heating rate of 0.3 ℃/min, and preserving heat for 8 hours; then reducing the temperature to 25 ℃ at the speed of 1 ℃/min; finally obtaining the ITWO target material; oxygen is introduced in the aerobic sintering process, and the flow rate of the oxygen is 50-100L/min.
Test example 1 Performance test
Test standards: measuring the density by adopting an Archimedes drainage method, and calculating to obtain the relative density by taking the true density as a reference; measuring the bending strength by adopting a three-point bending resistance method; measuring the resistivity of the target by a probe method;
and (3) test results: as shown in table 1:
TABLE 1 test results
As can be seen from Table 1, the ITWO target material prepared by the invention has the relative density of more than 95%, the target material purity of 99.99%, the average grain size of 10-15 um, the bending strength of more than or equal to 80MPa and good conductivity.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. An ITWO target, comprising an oxidized metal composition, the oxidized metal composition comprising: indium oxide, tin oxide, and tungsten oxide; tungsten oxide accounts for 1-5% of the total mass of the indium oxide and the tin oxide; the preparation process of the ITWO target material comprises the following steps: and (3) forming the oxidized metal composition compact and sintering.
2. The ITWO target of claim 1, wherein the mass ratio of indium oxide to tin oxide is: indium oxide: tin oxide is 9: 1.
3. A method of preparing an ITWO target material according to claim 1 or 2, comprising the steps of:
(1) mixing indium oxide and tin oxide according to a mass ratio, adding deionized water, and performing ball milling to obtain ITO slurry; adding tungsten oxide with corresponding mass into deionized water, and performing ball milling to obtain tungsten oxide slurry;
(2) adding tungsten oxide slurry into ITO slurry, adding a binder and a pH regulator, uniformly stirring to obtain mixed slurry, and drying to obtain ITWO powder;
(3) and forming an ITWO powder compact to obtain a biscuit, and sequentially carrying out degreasing sintering, aerobic sintering and anaerobic sintering on the biscuit to obtain the ITWO target material.
4. The method of preparing an ITWO target according to claim 3, wherein in step (1), the ITO paste has a D50<0.5 μm and a half-width of < 0.5.
5. The method for preparing an ITWO target material according to claim 3, wherein in the step (2), the mass of the binder is 2 to 5% of the total mass of the mixed slurry of tungsten oxide and ITO, and the binder is a polyolefinic binder; the pH regulator is ammonia water, and the pH value of the mixed slurry after regulation is 9-10.
6. The method for preparing an ITWO target according to claim 3, wherein in the step (2), the drying is performed by spray drying; the drying temperature of spray drying is 240-260 ℃, and the feeding speed is 600-1000 mL/min; the particle size of the obtained ITWO powder is less than 200 microns, and the moisture content of the ITWO powder is 0.2-0.3%.
7. The method for preparing an ITWO target material according to claim 3, wherein in the step (3), the green compact is formed by: putting ITWO powder into a die, pressing at 50MPa, and cold isostatic pressing at 300-400MPa to obtain the product with density of 4.2-4.5g/cm3The biscuit of (1).
8. The method for preparing an ITWO target material according to claim 3, wherein in the step (3), the degreasing and sintering process comprises: placing the biscuit in a sintering furnace, heating to 150-400 ℃ at the heating rate of 0.1-0.5 ℃/min, and carrying out degreasing sintering at the oxygen flow of 50-100L/min;
the process of aerobic sintering is as follows: after degreasing and sintering the biscuit, heating to 500-1300 ℃ at the heating rate of 0.1-0.5 ℃/min to carry out multi-stage heat preservation and sintering, and preserving heat for 1-4h at each temperature stage; heating to 1580 ℃ of 1300 ℃ at the heating rate of 0.3-0.5 ℃/min, and carrying out multi-stage heat preservation sintering, wherein the heat preservation time of each temperature stage is 2-8 h; introducing oxygen in the aerobic sintering process, wherein the flow rate of the oxygen is 50-100L/min;
the oxygen-free sintering process comprises the following steps: stopping introducing oxygen after aerobic sintering, cooling to 1400 ℃ at a cooling speed of 0.2-0.5 ℃/min, and preserving heat for 2-3 hours; heating to the highest target temperature at a heating rate of 0.1-0.3 ℃/min, preserving heat for 3-5 hours, then cooling to 25 ℃ at a cooling rate of 1-3 ℃/min, and introducing no gas in the process;
the multi-stage heat preservation sintering comprises a plurality of temperature rising stages and heat preservation stages, the temperature rises sequentially, and the temperature difference between any two heat preservation stages is 50-400 ℃.
9. The method of claim 8, wherein the oxygen-free sintering process has a maximum target temperature of 1500-.
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